CN107761160B - A kind of electrolytic etching agent of high-strength invar microscopic structure and caustic solution - Google Patents
A kind of electrolytic etching agent of high-strength invar microscopic structure and caustic solution Download PDFInfo
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- CN107761160B CN107761160B CN201710943497.4A CN201710943497A CN107761160B CN 107761160 B CN107761160 B CN 107761160B CN 201710943497 A CN201710943497 A CN 201710943497A CN 107761160 B CN107761160 B CN 107761160B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a kind of electrolytic etching agent of strong invar microscopic structure and caustic solution, the volume parts of raw material are as follows: 1 part of perchloric acid, 3~9 parts of acetic acid.This corrosion agent prescription is not simple, easy to use, volatile, reusable, and corrosive effect is good, mutually can clearly indicate out by the matrix of high-strength invar and disperse educt.This method carries out electrolytic etching using invar as anode, and the metal components such as iron, nickel in invar matrix can be electrolysed prior to precipitated phase, it is ensured that guarantees the complete of precipitated phase while corroding matrix out.The method of the present invention can be while corroding clearly austenite grain boundary profile out, a large amount of tiny precipitated phase particles of Dispersed precipitate is complete on guarantee austenite grain inside and crystal boundary, phased soln, peeling phenomenon are precipitated caused by avoiding due to using chemical mordant, has preferable applicability for the invar under different processing and condition of heat treatment.
Description
Technical field
The invention belongs to metallographic electrolytic etching technical field, especially a kind of electrolytic etching agent of high-strength invar microscopic structure
And caustic solution.
Background technique
Invar alloy, also known as invar, because it has extremely low thermal expansion coefficient below Curie temperature, in accurate industry neck
Domain has a wide range of applications.As the industrial products such as aviation composite molding die and remote times of capacity transmission conducting wire are to height
Strong invar demand rises year by year, the development work in relation to high-strength invar, increasingly the height weight by enterprise and scientific research institutions
Depending on.So far, industrially improve the most effective technical method of invar intensity be, using cold working working hardening, in conjunction with
The carbide second phase particle precipitation strength of ag(e)ing process.Under age strengthened temper, due to the austenitic matrix of high-strength invar
It is different from corrosion resistance of the precipitated phase particle to chemical erosion agent, in addition the difference of invar ingredient, heat treatment and machining state, makes to obtain
The etching pit for obtaining the precipitated phase particle of intact matrix microscopic structure and clear pattern becomes difficult.
Known document report mainly uses chemical erosion Faxian to show the matrix of invar, but this method is for disperse phase
Showing has biggish defect.For example, Chinese patent application " the display Fe-36Ni invar alloy of application number 201510824955.3
Solidify the aggressive agent and its corrosion method of arborescent structure ", wherein using picric acid, anhydrous cupric chloride, dehydrated alcohol, hydrochloric acid and ten
Dialkyl benzene sulfonic acids sodium mixed solution as aggressive agent, heating water bath to after 50~60 DEG C for showing Fe-36Ni invar alloy
Solidify arborescent structure.Zheng Hongguang et al. is in " Zr is on Fe-36Ni invar alloy solidified structure and thermoplastic influence " (Beijing science and technology
College journal, 2014,36 (S1): 145-150) in paper, the iron chloride saturation alcoholic solution of heating is used to corrode invar containing Zr
Solidified structure, obtained preferable displaing micro tissue topography.Lu Dongzhu etc. is in " in-situ produced SiC particulate enhancing Fe-36Ni invar alloy
Microstructure and property " gone using 4g copper sulphate, 20mL hydrochloric acid and 20mL in (Metallic Functional Materials, 2014,21 (04): 9-13)
The mixed solution of ionized water has carried out etching pit to the invar alloy that in-situ produced SiC particulate enhances, and in metallographic microscope and SEM
Under observe TiC particle influence to invar alloy tissue be added.Yang Xiaohua etc. is " Ti is to Fe-Ni expansion alloy solidified structure
Influence " 1g KMnO is used in (material engineering, 2010 (09): 7-9)4 +10mL H2SO4+90mL H2The mixed solution pair of O
Invar alloy is corroded, and the as-cast structure and precipitated phase of invar are observed.Tu Yifan et al. is " Fe-Ni base high intensity is low
In the relationship of expansion alloy structure property and aging time " (Metallic Functional Materials, 2007,14 (03): 10-14) text, use
5g CuSO4, 25ml HCl and 15ml H2The mixed solution of O erodes aging state hand-drawn wire sample, has clearly shown not
With the variation of sample crystal grain under aging technique.Yuan Junping is in " influence of deformation and heat treatment to invar alloy microstructure and property "
In (Central South University, 2005), wang aqueous solution (dense HNO is used3: dense HCl=1:3) respectively to cold rolled annealed state and hot rolling aging state
Invar alloy corroded, it is shown that the tissue topography under different conditions.Cai Bo et al. " Rare-Earth Ce to containing Nb it is ultralow swollen
It is water-soluble with ferric trichloride hydrochloric acid in the influence of swollen alloy structure and field trash " (Metallic Functional Materials, 2013,20 (01): 8-12)
Liquid is electrolyte, to Fe-Ni invar alloy 20~30s of electrolytic etching containing Ce and Nb under 4~5V voltage, is obtained different containing Ce
As-forged microstructure under amount.However above-mentioned caustic solution is in the etching pit process to the invar alloy strengthened containing Second Phase Precipitation
In often will cause Second Phase Particle be etched liquid dissolution, a large amount of eroded crater is shown as under Electronic Speculum, seriously affects microcosmic shape
The constituent analysis of looks quality and precipitated phase.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of electrolysis of the good high-strength invar microscopic structure of corrosive effect corruption
Lose agent；The present invention also provides a kind of caustic solutions of high-strength invar microscopic structure.
In order to solve the above technical problems, the volume parts of raw material adopted by the present invention are as follows: 1 part of perchloric acid, acetic acid 3~9
Part.
Perchloric acid purity of the present invention is 70wt%~72wt%, acetic acid purity >=99.5wt%.
The method of the present invention uses above-mentioned electrolytic etching agent, processing step are as follows: (1) is played invar sample to be corroded
It is polished after mill；
(2) the invar sample after the polishing carries out electrolytic etching as anode in electrolytic etching agent；
(3) the invar sample by the invar sample wash after electrolytic etching, drying, after corrosion can be obtained.
In step described in the method for the present invention (2), the DC voltage of electrolytic etching is 20~30V, and electric current is 1.0~3A, temperature
Degree is 0~40 DEG C, and the time is 25~30s.
The beneficial effects of adopting the technical scheme are that inventive formulation it is simple, it is easy to use, be not easy to wave
Hair, reusable, corrosive effect is good, mutually can clearly indicate out by the matrix of high-strength invar and disperse educt.
The present invention carries out electrolytic etching using invar as anode, and the metal components such as iron, nickel in invar matrix can be preferential
It is electrolysed in precipitated phase, it is ensured that while corroding matrix out, guarantee the complete of precipitated phase.The method of the present invention can
With while corroding clearly austenite grain boundary profile out, Dispersed precipitate is big on guarantee austenite grain inside and crystal boundary
The complete of tiny precipitated phase particle is measured, phased soln, peeling phenomenon are precipitated caused by avoiding due to using chemical mordant, it is right
Invar under different processing and condition of heat treatment has preferable applicability.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is that embodiment 1 corrodes obtained high-strength invar hand-drawn wire through aging state SEM photograph；
Fig. 2 is that embodiment 3 corrodes obtained high-strength invar hand-drawn wire through aging state SEM photograph；
Fig. 3 is that embodiment 5 corrodes obtained high-strength invar gren rod radial direction SEM photograph；
Fig. 4 is that the high-strength invar hot rolled plate that the corrosion of embodiment 8 obtains is rolled to SEM photograph；
Fig. 5 is to roll after embodiment 10 corrodes obtained high-strength invar hot rolled plate ageing treatment to SEM photograph；
Fig. 6 is the high-strength invar hand-drawn wire that corrodes of comparative example through aging state SEM photograph.
Specific embodiment
Following Examples 1 to 4 are the electrolytic etching process of high-strength invar hand-drawn wire aged.
Embodiment 1: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
(1) it prepares electrolytic etching agent: measuring acetic acid 50ml, acetic acid 450ml, acetic acid is first poured into glass container at room temperature
In, then perchloric acid is poured into acetic acid, and is stirred evenly with glass bar.
(2) it by after the high-strength invar H36 hand-drawn wire ageing treatment corroded, radially samples, and polished with silicon carbide paper,
It is mechanically polished again with diamond polishing agent.
(3) the electrolytic etching agent that step (1) is prepared is poured into electrolytic etching instrument, the cathode material of electrolytic etching instrument uses
The sample after step (2) polishing is carried out electrolytic etching, DC voltage 30V, electric current 2.5A, electrolysis by 304 stainless steels
Corrosion temperature is 0 DEG C, the electrolytic etching time is 30s.
(4) sample is taken out from corrosive agent, is rinsed well again with dehydrated alcohol after being rinsed using deionized water, with blowing
Machine drying, the invar sample after corrosion can be obtained.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, SEM photograph is shown in Fig. 1；By Fig. 1
As it can be seen that its surface shows intact matrix microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 2: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 50ml, acetic acid 450ml；After high-strength invar H36 hand-drawn wire ageing treatment, edge
Radial sampling；Electrolytic corrosion process: DC voltage 30V, electric current 2A, temperature be 0 DEG C, time 30s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, surface shows complete base
Body microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 3: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 400ml；After high-strength invar H36 hand-drawn wire ageing treatment, edge
Axial sampling；Electrolytic corrosion process: DC voltage 25V, electric current 1.8A, temperature be 8 DEG C, time 25s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, SEM photograph is shown in Fig. 2；By Fig. 2
As it can be seen that its surface shows intact matrix microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 4: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 300ml；After high-strength invar H36 hand-drawn wire ageing treatment, edge
Axial sampling；Electrolytic corrosion process: DC voltage 20V, electric current 2A, temperature be 12 DEG C, time 28s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, surface shows complete base
Body microscopic structure and clearly pattern, and only a small amount of eroded crater.
Following embodiments 5,6 are the electrolytic etching process of high-strength invar gren rod.
Embodiment 5: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 50ml, acetic acid 450ml；High-strength invar H36 gren rod radially samples；
Electrolytic corrosion process: DC voltage 30V, electric current 3A, temperature be 19 DEG C, time 30s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, SEM photograph is shown in Fig. 3；By Fig. 3
As it can be seen that its surface shows intact matrix microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 6: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 400ml；High-strength invar H36 gren rod radially samples；
Electrolytic corrosion process: DC voltage 25V, electric current 2.1A, temperature be 23 DEG C, time 25s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, surface shows complete base
Body microscopic structure and clearly pattern, and only a small amount of eroded crater.
Following embodiments 7~10 are the electrolytic etching process under high-strength invar hot rolled plate and hot rolled plate difference aged.
Embodiment 7: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 50ml, acetic acid 450ml；It rolls to sampling on high-strength invar H36 hot rolled plate edge；Electricity
Solve etching process: DC voltage 30V, electric current 2A, temperature be 25 DEG C, time 25s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, surface shows complete base
Body microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 8: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 400ml；It rolls to sampling on high-strength invar H36 hot rolled plate edge；Electricity
Solve etching process: DC voltage 30V, electric current 1.5A, temperature be 28 DEG C, time 30s.Remaining is the same as embodiment 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, SEM photograph is shown in Fig. 4；By Fig. 4
As it can be seen that its surface shows intact matrix microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 9: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 400ml；High-strength invar H36 hot rolled plate after ageing treatment,
Radially sample；Electrolytic corrosion process: DC voltage 25V, electric current 2.3A, temperature be 32 DEG C, time 25s.Remaining is the same as implementation
Example 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, surface shows complete base
Body microscopic structure and clearly pattern, and only a small amount of eroded crater.
Embodiment 10: the caustic solution of this high-strength invar microscopic structure uses following concrete technologies.
It prepares electrolytic etching agent: measuring acetic acid 100ml, acetic acid 300ml；High-strength invar H36 hot rolled plate after ageing treatment,
Radially sample；Electrolytic corrosion process: DC voltage 20V, electric current 1.0A, temperature be 40 DEG C, time 25s.Remaining is the same as implementation
Example 1.
Using the invar sample after corrosion obtained by field emission microscopy observation corrosion surface, SEM photograph is shown in Fig. 5；By Fig. 5
As it can be seen that its surface shows intact matrix microscopic structure and clearly pattern, and only a small amount of eroded crater.
Comparative example: high-strength invar hand-drawn wire is after aging state, using liquor ferri trichloridi as corrosive agent, using conventional gold
Phase caustic solution is corroded, and the SEM photograph of sample is shown in Fig. 6 after corrosion；As seen from Figure 6, there is a large amount of eroded crater on surface, the
Two-phase particle be corroded liquid dissolution, seriously affect the constituent analysis of microscopic appearance quality and precipitated phase.
Claims (2)
1. a kind of caustic solution of high-strength invar microscopic structure, the volume parts of electrolytic etching agent raw material are as follows: 1 part of perchloric acid, vinegar
3~9 parts of acid, the perchloric acid purity are 70wt%~72wt%, acetic acid purity >=99.5wt%, which is characterized in that its processing step
Are as follows: (1) the invar sample wait corrode is polished after polishing；
(2) the invar sample after the polishing carries out electrolytic etching as anode in electrolytic etching agent；
(3) the invar sample by the invar sample wash after electrolytic etching, drying, after corrosion can be obtained.
2. the caustic solution of high-strength invar microscopic structure according to claim 1, it is characterised in that: in the step (2),
The DC voltage of electrolytic etching is 20~30V, and electric current is 1.0~3A, and temperature is 0~40 DEG C, and the time is 25~30s.
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| CN109991254A (en) * | 2019-04-29 | 2019-07-09 | 福建工程学院 | A kind of preparation method of pure iron EBSD sample |
| CN110085337B (en) * | 2019-05-20 | 2020-09-08 | 中国核动力研究设计院 | UO2-ZrO2Preparation method of sample for microstructure analysis of ceramic fuel |
| CN110453222B (en) * | 2019-08-08 | 2021-07-13 | 重庆科技学院 | Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof |
| CN111676508B (en) * | 2020-05-14 | 2021-12-14 | 天津大学 | Electrolytic corrosion solution and application thereof |
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